US5030494A - Carbon overcoat for a thin film magnetic recording disk containing discrete clusters of tungsten (W) or tungsten carbide (WC) which project from the surface of the overcoat - Google Patents
Carbon overcoat for a thin film magnetic recording disk containing discrete clusters of tungsten (W) or tungsten carbide (WC) which project from the surface of the overcoat Download PDFInfo
- Publication number
- US5030494A US5030494A US07/302,844 US30284489A US5030494A US 5030494 A US5030494 A US 5030494A US 30284489 A US30284489 A US 30284489A US 5030494 A US5030494 A US 5030494A
- Authority
- US
- United States
- Prior art keywords
- overcoat
- disk
- carbon
- thin film
- tungsten
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 24
- 239000010409 thin film Substances 0.000 title claims abstract description 20
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 13
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000010937 tungsten Substances 0.000 title claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 23
- 239000010408 film Substances 0.000 claims abstract description 20
- 229910001092 metal group alloy Inorganic materials 0.000 claims abstract description 9
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 23
- 150000001721 carbon Chemical class 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 229910000531 Co alloy Inorganic materials 0.000 claims description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
- 229910000838 Al alloy Inorganic materials 0.000 claims 2
- 239000000654 additive Substances 0.000 abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 239000011651 chromium Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- HBXWYZMULLEJSG-UHFFFAOYSA-N chromium vanadium Chemical compound [V][Cr][V][Cr] HBXWYZMULLEJSG-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010702 perfluoropolyether Substances 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/72—Protective coatings, e.g. anti-static or antifriction
- G11B5/727—Inorganic carbon protective coating, e.g. graphite, diamond like carbon or doped carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer
Definitions
- This invention relates to a thin film metal alloy magnetic recording disk, and in particular to such a disk having a protective overcoat of a metal-containing or metal carbide-containing carbon film.
- the invention also relates to a contact start/stop (CSS) rigid disk file having such a disk as the magnetic recording medium.
- CSS contact start/stop
- each of the read/write transducers or heads is supported on a slider which rides on a cushion or bearing of air above the surface of the disk when the disk is rotating at its operating speed.
- the slider is connected to a linear or rotary voice coil actuator by means of a relatively fragile suspension.
- a thin film metal alloy disk which typically comprises a substrate, such as an aluminum-magnesium (AlMg) alloy with a nickel-phosphorous (NiP) surface coating, a cobalt-based alloy sputter deposited as the magnetic layer on the substrate, and a protective overcoat, such as a sputter-deposited amorphous carbon film, formed on the magnetic layer.
- AlMg aluminum-magnesium
- NiP nickel-phosphorous
- a protective overcoat such as a sputter-deposited amorphous carbon film
- Amorphous hydrogenated carbon films formed by reactive sputtering of a graphite target in an atmosphere of argon and hydrocarbon gases have been suggested as suitable for use as thin film disk protective overcoats, as described in Japanese Kokai No. 60-157725. Assignee's U.S. Pat. No.
- thin film disks may also include a sputter-deposited underlayer, such as a layer of chromium (Cr), chromium-vanadium (CrV) or tungsten (W), between the substrate and the magnetic layer and a sputter deposited adhesion layer, such as a Cr, W or titanium (Ti) layer, between the magnetic layer and the protective overcoat.
- a sputter-deposited underlayer such as a layer of chromium (Cr), chromium-vanadium (CrV) or tungsten (W)
- Cr chromium-vanadium
- Ti titanium
- an additional problem in disk files which use thin film disks is the suitability of the protective overcoat to provide resistance to wear caused by contact of the disk by the air-bearing slider which carries the magnetic recording head.
- the invention is a thin film metal alloy magnetic recording disk having an improved protective overcoat which is both wear resistant and which creates a low level of stiction in a CSS disk file.
- the overcoat is a film of essentially amorphous carbon or hydrogen-containing carbon with relatively small amounts of embedded iron (Fe), tungsten (W) or tungsten-carbide (WC).
- Fe embedded iron
- W tungsten
- WC tungsten-carbide
- the protective overcoat has a relatively smooth planar carbon surface with discrete clusters of the additives which project slightly above the smooth carbon surface. It is this particular characteristic of the protective overcoat which is believed responsible for the low static friction.
- the present invention is also directed to a rigid disk file of the CSS type wherein the thin film metal alloy disks have the above-described protective overcoat.
- FIGS. 1(a) and (b) are atomic force microscope (AFM) micrographs of the surface topographies of an amorphous hydrogenated carbon film with and without W impregnated in the film;
- FIGS. 2(a) and (b) are plots of initial stiction (in grams) as a function of CSS cycles on W impregnated amorphous hydrogenated carbon films formed on a polished Si substrate, and on a polished NiP substrate with a W underlayer;
- FIGS. 3(a) and (b) are plots of initial stiction (in grams) as a function of CSS cycles for a tungsten carbide (WC) impregnated amorphous hydrogenated carbon film formed on textured NiP substrate, and for an amorphous hydrogenated carbon film without WC formed on a textured NiP substrate.
- WC tungsten carbide
- the thin film disks were fabricated in a Sputtered Films Inc. (SFI) s-gun magnetron sputtering system, using planetary rotation.
- the disk structure consisted of an underlayer (200-300 Angstroms Cr), a magnetic layer (300-500 Angstroms CoPtCr or CoNiCr), an adhesion sublayer ( ⁇ 50 Angstroms W, Ti or Ta) and a carbon-based overcoat (200 Angstroms).
- the disks were deposited on substrates of smooth single-crystal silicon (Si) and on both polished and textured AlMg/NiP.
- the recording metal layer was deposited using DC magnetron sputtering, whereas the overcoat layers were deposited using either DC or RF sputtering.
- a substrate bias voltage (-50V) was applied during the deposition of the underlayers and the sublayers to promote film adhesion.
- the magnetic layers and the overcoats were deposited with no substrate bias.
- Metal additives Si, Ti, Ta and W
- carbide additives TiC, TaC and WC
- concentration of additive in the overcoat was estimated from the calibrated relative deposition rates of the materials from the sputtering targets.
- the disks were then treated with 20-30 Angstroms of conventional lubricant, such as perfluoropolyethers applied by dip coating or spraying.
- AHT accelerated wear tests
- a protective overcoat of an amorphous carbon film with Fe embedded in the carbon film was fabricated by DC magnetron sputter deposition of a graphite target, with an iron strip near the racetrack, in an Ar atmosphere.
- the resulting amorphous carbon with impregnated Fe also exhibited low friction and high durability.
- the low friction and high durability caused by the embedded Fe would also result if the Fe were embedded in an amorphous hydrogenated carbon overcoat.
- FIG. 1(b) there is shown a micrograph by an Atomic Force Microscope (AFM) which illustrates the surface topography of a hydrogenated carbon overcoat of 200 Angstroms thickness with no metal or metal carbide particles present.
- AFM Atomic Force Microscope
- FIG. 1(a) there is a similar AFM micrograph of a protective overcoat of a hydrogenated carbon film with 6% W.
- peaks having a height of approximately 60 Angstrom which are believed to be microcrystaline clusters of W projecting from the substantially planar carbon surface. It is this "microroughness" characteristic of the protective overcoat which is believed to produce the low initial static friction. This microroughness has also been observed for the overcoats with embedded WC.
- FIGS. 3(a) and (b) establish that stiction improvement can be achieved by sputtering the overcoat from a single target and can benefit thin film disks using textured substrates.
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Magnetic Record Carriers (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
TABLE 1
______________________________________
Stiction Durability
Test Overcoat (gms) (CSS cycles) AWT Cycles
______________________________________
1 H--C >45 >10,000 60-90,000
2 H--C/4.2% Si >50 0
3 H--C/7.8% Si >50 0
4 H--C/10.0% Ti
20-40 ˜3,000
5 H--C/4-7% Ta 4-20 ˜4,000
6 H--C/4-8% W 5-8 >10,000
7 H--C/3.2% TiC
˜10
˜300
8 H--C/8.5% TaC
˜8
˜1,000
9 H--C/4-10% WC
5-10 >10,000 >500,000
______________________________________
Claims (6)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/302,844 US5030494A (en) | 1989-01-26 | 1989-01-26 | Carbon overcoat for a thin film magnetic recording disk containing discrete clusters of tungsten (W) or tungsten carbide (WC) which project from the surface of the overcoat |
| DE69024379T DE69024379T2 (en) | 1989-01-26 | 1990-01-25 | Carbon coating for a magnetic thin film recording plate |
| EP90850035A EP0381652B1 (en) | 1989-01-26 | 1990-01-25 | An improved carbon overcoat for a thin film magnetic recording disc |
| JP2015135A JPH0766540B2 (en) | 1989-01-26 | 1990-01-26 | Thin film magnetic disk |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/302,844 US5030494A (en) | 1989-01-26 | 1989-01-26 | Carbon overcoat for a thin film magnetic recording disk containing discrete clusters of tungsten (W) or tungsten carbide (WC) which project from the surface of the overcoat |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US5030494A true US5030494A (en) | 1991-07-09 |
Family
ID=23169452
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US07/302,844 Expired - Lifetime US5030494A (en) | 1989-01-26 | 1989-01-26 | Carbon overcoat for a thin film magnetic recording disk containing discrete clusters of tungsten (W) or tungsten carbide (WC) which project from the surface of the overcoat |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US5030494A (en) |
| EP (1) | EP0381652B1 (en) |
| JP (1) | JPH0766540B2 (en) |
| DE (1) | DE69024379T2 (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5271802A (en) * | 1990-12-27 | 1993-12-21 | International Business Machines Corporation | Method for making a thin film magnetic head having a protective coating |
| US5486276A (en) * | 1992-09-10 | 1996-01-23 | Fujitsu Limited | Method for manufacturing small magnetic disks from a large disk |
| US5562982A (en) * | 1992-09-30 | 1996-10-08 | Matsushita Electric Industrial Co., Ltd. | Magnetic recording medium |
| US5569506A (en) * | 1993-10-06 | 1996-10-29 | International Business Machines Corporation | Magnetic recording disk and disk drive with improved head-disk interface |
| US5705287A (en) * | 1994-09-20 | 1998-01-06 | International Business Machines Corporation | Magnetic recording disk with metal nitride texturing layer |
| US5773124A (en) * | 1993-02-22 | 1998-06-30 | Hitachi, Ltd. | Magnetic recording medium comprising a protective layer having specified electrical resistivity and density |
| US5949612A (en) * | 1995-03-21 | 1999-09-07 | Censtor Corp. | Low friction sliding hard disk drive system |
| US6171676B1 (en) | 1996-03-19 | 2001-01-09 | Fujitsu Limited | Magnetic recording medium containing fine magnetic crystal grains and its manufacture |
| US6522501B1 (en) * | 1999-12-28 | 2003-02-18 | Kabushiki Kaisha Toshiba | Magnetic recording medium and magnetic write/read apparatus using the same |
| US6638622B2 (en) | 2001-01-11 | 2003-10-28 | Hitachi Global Storage Technologies | Perfluorinated polyethers with metal carboxylate end groups as anti-wetting and corrosion-protective agents |
| US6804085B1 (en) * | 1995-03-21 | 2004-10-12 | Seagate Technology, Llc | Hard drive system interface between a disk surface and a transducer contacting the surface during communication |
| US20090178905A1 (en) * | 2005-07-15 | 2009-07-16 | Abb Research Ltd. | Contact Element and a Contact Arrangement |
Citations (17)
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|---|---|---|---|---|
| US3912461A (en) * | 1970-11-02 | 1975-10-14 | Texas Instruments Inc | Low temperature metal carbonitride coatings |
| JPS5961106A (en) * | 1982-09-30 | 1984-04-07 | Nec Corp | Magnetic memory body |
| US4525417A (en) * | 1982-02-27 | 1985-06-25 | U.S. Philips Corporation | Carbon-containing sliding layer |
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| US4675240A (en) * | 1982-11-22 | 1987-06-23 | International Business Machines Corporation | Magnetic recording disk using silicon substrate |
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| JPS63102014A (en) * | 1986-10-17 | 1988-05-06 | Fuji Photo Film Co Ltd | Magnetic recording medium |
| US4778582A (en) * | 1987-06-02 | 1988-10-18 | International Business Machines Corporation | Process for making a thin film metal alloy magnetic recording disk with a hydrogenated carbon overcoat |
| US4789913A (en) * | 1987-08-03 | 1988-12-06 | International Business Machines Corporation | Method and apparatus for lubricating a magnetic disk continuously in a recording file |
| US4840843A (en) * | 1986-10-17 | 1989-06-20 | Fuji Photo Film Co., Ltd. | Magnetic recording medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63217518A (en) * | 1987-03-05 | 1988-09-09 | Fuji Photo Film Co Ltd | Magnetic recording medium |
-
1989
- 1989-01-26 US US07/302,844 patent/US5030494A/en not_active Expired - Lifetime
-
1990
- 1990-01-25 DE DE69024379T patent/DE69024379T2/en not_active Expired - Fee Related
- 1990-01-25 EP EP90850035A patent/EP0381652B1/en not_active Expired - Lifetime
- 1990-01-26 JP JP2015135A patent/JPH0766540B2/en not_active Expired - Fee Related
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| US4578729A (en) * | 1981-10-15 | 1986-03-25 | Matsushita Electric Industrial Co., Ltd. | Magnetic recording medium |
| US4525417A (en) * | 1982-02-27 | 1985-06-25 | U.S. Philips Corporation | Carbon-containing sliding layer |
| JPS5961106A (en) * | 1982-09-30 | 1984-04-07 | Nec Corp | Magnetic memory body |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5271802A (en) * | 1990-12-27 | 1993-12-21 | International Business Machines Corporation | Method for making a thin film magnetic head having a protective coating |
| US5486276A (en) * | 1992-09-10 | 1996-01-23 | Fujitsu Limited | Method for manufacturing small magnetic disks from a large disk |
| US5552203A (en) * | 1992-09-10 | 1996-09-03 | Fujitsu Limited | Magnetic disk having a protective layer of sputtered particles of two differently controlled grain sizes |
| US5562982A (en) * | 1992-09-30 | 1996-10-08 | Matsushita Electric Industrial Co., Ltd. | Magnetic recording medium |
| US5679454A (en) * | 1992-09-30 | 1997-10-21 | Matsushita Electric Industrial Co., Ltd. | Magnetic recording medium |
| US5773124A (en) * | 1993-02-22 | 1998-06-30 | Hitachi, Ltd. | Magnetic recording medium comprising a protective layer having specified electrical resistivity and density |
| US5569506A (en) * | 1993-10-06 | 1996-10-29 | International Business Machines Corporation | Magnetic recording disk and disk drive with improved head-disk interface |
| US5705287A (en) * | 1994-09-20 | 1998-01-06 | International Business Machines Corporation | Magnetic recording disk with metal nitride texturing layer |
| US6804085B1 (en) * | 1995-03-21 | 2004-10-12 | Seagate Technology, Llc | Hard drive system interface between a disk surface and a transducer contacting the surface during communication |
| US5949612A (en) * | 1995-03-21 | 1999-09-07 | Censtor Corp. | Low friction sliding hard disk drive system |
| US6171676B1 (en) | 1996-03-19 | 2001-01-09 | Fujitsu Limited | Magnetic recording medium containing fine magnetic crystal grains and its manufacture |
| US6522501B1 (en) * | 1999-12-28 | 2003-02-18 | Kabushiki Kaisha Toshiba | Magnetic recording medium and magnetic write/read apparatus using the same |
| US6638622B2 (en) | 2001-01-11 | 2003-10-28 | Hitachi Global Storage Technologies | Perfluorinated polyethers with metal carboxylate end groups as anti-wetting and corrosion-protective agents |
| US20040021984A1 (en) * | 2001-01-11 | 2004-02-05 | Qing Dai | Magnetic recording head having a corrosion-protective layer of a metal salt of a perfluorinated polyether acid |
| US20040023033A1 (en) * | 2001-01-11 | 2004-02-05 | Qing Dai | Method for making a magnetic recording disk having a corrosion-protective layer of a perfluorinated polyether acid |
| US20040023076A1 (en) * | 2001-01-11 | 2004-02-05 | Qing Dai | Process for synthesizing perfluorinated polyethers with metal carboxylate end groups |
| US6916955B2 (en) | 2001-01-11 | 2005-07-12 | International Business Machines | Process for synthesizing perfluorinated polyethers with metal carboxylate end groups |
| US6932890B2 (en) | 2001-01-11 | 2005-08-23 | International Business Machines Corporation | Method for making a magnetic recording disk having a corrosion-protective layer of a perfluorinated polyether acid |
| US6940692B2 (en) | 2001-01-11 | 2005-09-06 | International Business Machines | Magnetic recording head having a corrosion-protective layer of a metal salt of a perfluorinated polyether acid |
| US20090178905A1 (en) * | 2005-07-15 | 2009-07-16 | Abb Research Ltd. | Contact Element and a Contact Arrangement |
| US7709759B2 (en) * | 2005-07-15 | 2010-05-04 | Abb Research Ltd. | Contact element and a contact arrangement |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02230510A (en) | 1990-09-12 |
| JPH0766540B2 (en) | 1995-07-19 |
| DE69024379T2 (en) | 1996-07-18 |
| EP0381652A2 (en) | 1990-08-08 |
| DE69024379D1 (en) | 1996-02-08 |
| EP0381652B1 (en) | 1995-12-27 |
| EP0381652A3 (en) | 1991-05-29 |
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